Hydrochloric Acid → 3-Ethylthio-2-methyl-4-trifluoromethylbenzoic acid

HRID 2079561

Reaktionsgleichung

Reaktionsgleichung von HRID 2079561
F[C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[C:5]([OH:7])=[O:6].[H-].[Na+].[CH2:18]([SH:20])[CH3:19].Cl>CN(C)C=O>[CH2:18]([S:20][C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[C:5]([OH:7])=[O:6])[CH3:19]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 6343EthanethiolHCID 24758Sodium hydrideHCID 574577653-Fluoro-2-methyl-4-(trifluoromethyl)benzoic acid

Produkt 1

HCID 574577663-Ethylthio-2-methyl-4-trifluoromethylbenzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

3.00 g (13.5 mmol) of 3-fluoro-2-methyl-4-trifluoromethylbenzoic acid were initially charged in 50 ml of N,N-dimethylformamide. 1.68 g (purity 60% by weight, 41.9 mmol) of NaH were added a little at a time. Towards the end of the evolution of gas, 1.77 g (purity 95% by weight, 27.0 mmol) of ethanethiol were added dropwise. The mixture was stirred at RT for 2 h and then heated at 80° C. for 10 h. The reaction mixture was cooled and, for workup, poured into ice-water and then acidified with concentrated hydrochloric acid. The product precipitated out and was separated off by filtration. What was isolated were 3.7 g of the pure product.

Aufarbeitung

  1. temperatureheated at 80° C. for 10 h
  2. temperatureThe reaction mixture was cooled and, for workup
  3. customThe product precipitated out
  4. customwas separated off by filtration
  5. customWhat was isolated

Quellen und Nachweise

ORD-Eintrag
ord-f061d0f85d7f4d7a90b5462c457cdf73
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07932211B2

Verknüpfte Notizen

Wird geladen…